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Dear Gerd,
> I'm trying to set up an HPLC method for analysis
> of pah in soil. Everything is working fine, now I
> want to change from UV to fl detection. I have
> a Kratos 980, which allows programming of the excitation
> wavelength, but not the emission wavelength. All publications
you want to to find only the 16 priority PAHs ? or extended list ?
(1)
try to set the excitation wavelength according to their lambda max.
(similar to their maximum in the UV-spectra) - if you have a strong
"baseline jumping" during wavelength switching - group your
molecules - like:
280 nm - Naphthalene, Acenaphtylene, Acenaphthene,Fluorene
250 nm - Phenanthrene,Anthracene
260 nm - Fluoranthene,Pyrene
265 nm - Benzo[a]anthracene,Chrysene
305 nm - Benzo[b]fluoranthene,Benzo[k]fluoranthene,
Benzo[a]pyrene,Dibenz[a,h]anthracene,Benzo[g,h,i]perylene,
Indeno[1,2,3-cd]pyrene
(2)
set your (fixed) emission wavelength to 335 nm for the first run
for the first 5-6 PAHs
set your (fixed) emission wavelength to 420 nm for the second run
for the rest
(2.1) Why 2 runs ? This is the price for a high sensitivity.
(A) from a monetary point of view I would say if you have to
do a lot of runs - try to get a exc./em. switchable device :-)
(B) from a chemometrical point of view I nevertheless suggest
to do 8 runs with settings from (1) and try emission wavelength
from 320 nm to 480 nm (20 nm steps).
This will take one day or night and will solve your problem in the best
way
(solvent, sensitivity,column, number of PAHs).
(C) Beware - this is not trivial - you will even lose some molecules
with 2 runs because PAHs also have different emission intensities.
For further reading:
(These publications have all pictures from fluorescence spectra and
listed
excitation and emission wavelengths and will also list some "uncommon"
PAHs - I write this because there are millions of PAH publications...)
*Investigation on simultaneous analysis of multicomponent polycyclic
aromatic hydrocarbon mixtures in water samples: a simple synchronous
fluorimetric method, Talanta, Volume 55, Issue 1, 3 August 2001, Pages
143-153
Digambara Patra and A. K. Mishra
*Fluorescence spectroscopy of aromatic species produced in rich
premixed ethylene flames, Chemosphere, Volume 42, Issues 5-7,
February 2001, Pages 835-841 A. Ciajolo, R. Ragucci, B. Apicella,
R. Barbella, M. de Joannon and A. Tregrossi
*Fish Biliary Polycyclic Aromatic Hydrocarbon Metabolites Estimated
by Fixed-Wavelength Fluorescence: Comparison
with HPLC-Fluorescent Detection
EDITH L. C. LIN,SUSAN M. CORMIER, AND JONI A. TORSELLA
ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY 35, 16–23 (1996)
*Invited Review
Photochemistry and Photobiology, Vol. 70, Iss. 1, July 1999
A Compilation of Physical, Spectroscopic and Photophysical Properties of
Polycyclic Aromatic Hydrocarbons
Reza Dabestani* and Ilia N. Ivanov
http://www.pol-us.net/PAPHome/Vol70/pdfs/vol70iss1pp10-34.pdf
*Investigation on simultaneous analysis of multicomponent
polycyclic aromatic hydrocarbon mixtures in water samples:
a simple synchronous fluorimetric method
Talanta 55 (2001) 143–153
Digambara Patra, A.K. Mishra
With kind regards
Tobias Kind
PS:
Try also the NIST (Sander/Wise)
"Polycyclic Aromatic Hydrocarbon Structure Index"
http://ois.nist.gov/pah/
and
the Jinno Lab Polycyclic Aromatic Hydrocarbons (PAHs) Data Base
http://chrom.tutms.tut.ac.jp/JINNO/DATABASE/00database.html
and if you want to see their nice Kirschbaumbluetenfest (o-hanami) take
http://chrom.tutms.tut.ac.jp/JINNO/Memory/memory_frame.html
...ooops they cutted their last pictures - hope they had no
"sake excess" - just kidding :-)
Tobias Kind wrote:
>
> Dear Gerd,
>
> > I'm trying to set up an HPLC method for analysis
> > of pah in soil. Everything is working fine, now I
> > want to change from UV to fl detection. I have
> > a Kratos 980, which allows programming of the excitation
> > wavelength, but not the emission wavelength. All publications
>
> you want to to find only the 16 priority PAHs ? or extended list ?
>
> (1)
> try to set the excitation wavelength according to their lambda max.
> (similar to their maximum in the UV-spectra) - if you have a strong
> "baseline jumping" during wavelength switching - group your
> molecules - like:
> 280 nm - Naphthalene, Acenaphtylene, Acenaphthene,Fluorene
> 250 nm - Phenanthrene,Anthracene
> 260 nm - Fluoranthene,Pyrene
> 265 nm - Benzo[a]anthracene,Chrysene
> 305 nm - Benzo[b]fluoranthene,Benzo[k]fluoranthene,
> Benzo[a]pyrene,Dibenz[a,h]anthracene,Benzo[g,h,i]perylene,
>
> Indeno[1,2,3-cd]pyrene
> (2)
> set your (fixed) emission wavelength to 335 nm for the first run
> for the first 5-6 PAHs
> set your (fixed) emission wavelength to 420 nm for the second run
> for the rest
>
> (2.1) Why 2 runs ? This is the price for a high sensitivity.
>
> (A) from a monetary point of view I would say if you have to
> do a lot of runs - try to get a exc./em. switchable device :-)
>
> (B) from a chemometrical point of view I nevertheless suggest
> to do 8 runs with settings from (1) and try emission wavelength
> from 320 nm to 480 nm (20 nm steps).
> This will take one day or night and will solve your problem in the best
> way
> (solvent, sensitivity,column, number of PAHs).
>
> (C) Beware - this is not trivial - you will even lose some molecules
> with 2 runs because PAHs also have different emission intensities.
>
> For further reading:
> (These publications have all pictures from fluorescence spectra and
> listed
> excitation and emission wavelengths and will also list some "uncommon"
> PAHs - I write this because there are millions of PAH publications...)
>
> *Investigation on simultaneous analysis of multicomponent polycyclic
> aromatic hydrocarbon mixtures in water samples: a simple synchronous
> fluorimetric method, Talanta, Volume 55, Issue 1, 3 August 2001, Pages
> 143-153
> Digambara Patra and A. K. Mishra
>
> *Fluorescence spectroscopy of aromatic species produced in rich
> premixed ethylene flames, Chemosphere, Volume 42, Issues 5-7,
> February 2001, Pages 835-841 A. Ciajolo, R. Ragucci, B. Apicella,
> R. Barbella, M. de Joannon and A. Tregrossi
>
> *Fish Biliary Polycyclic Aromatic Hydrocarbon Metabolites Estimated
> by Fixed-Wavelength Fluorescence: Comparison
> with HPLC-Fluorescent Detection
> EDITH L. C. LIN,SUSAN M. CORMIER, AND JONI A. TORSELLA
> ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY 35, 16–23 (1996)
>
> *Invited Review
> Photochemistry and Photobiology, Vol. 70, Iss. 1, July 1999
> A Compilation of Physical, Spectroscopic and Photophysical Properties of
>
> Polycyclic Aromatic Hydrocarbons
> Reza Dabestani* and Ilia N. Ivanov
> http://www.pol-us.net/PAPHome/Vol70/pdfs/vol70iss1pp10-34.pdf
>
> *Investigation on simultaneous analysis of multicomponent
> polycyclic aromatic hydrocarbon mixtures in water samples:
> a simple synchronous fluorimetric method
> Talanta 55 (2001) 143–153
> Digambara Patra, A.K. Mishra
>
> With kind regards
> Tobias Kind
>
> PS:
> Try also the NIST (Sander/Wise)
> "Polycyclic Aromatic Hydrocarbon Structure Index"
> http://ois.nist.gov/pah/
>
> and
> the Jinno Lab Polycyclic Aromatic Hydrocarbons (PAHs) Data Base
> http://chrom.tutms.tut.ac.jp/JINNO/DATABASE/00database.html
>
> and if you want to see their nice Kirschbaumbluetenfest (o-hanami) take
> http://chrom.tutms.tut.ac.jp/JINNO/Memory/memory_frame.html
>
> ...ooops they cutted their last pictures - hope they had no
> "sake excess" - just kidding :-)
Thanks a lot!
I try to find "only" the 16 PAH's. I used UV detection before,
which runs pretty good, but I recently got a used FL detector
and so I thought I can use it to increase sensitivity. A new
one is not possible.
The students can't do two runs of each sample, so I have
to find out a way with switching only the ex wavelength.
The german DIN method suggests 365/470 nm, but I found the results
were really bad. (Maybe I have to use a xenon lamp instead of
the D2 one, but I don't have the power supply for it).
Best results up to now are something like 270/340 nm using
a cut-off filter (which allows detection of all emissions
above about 340 nm.)
Thanks also for the links. BTW - Agilent has a nice PAH handbook
in pdf available with all spectra on their hompepage.
Kind regards,
Gerd Klaassen
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